Utilization of biowaste eggshells to synthesize nanocrystalline hydroxyapatite powders

Nano hydroxyapatite (HA) powder was successfully synthesized from biowaste chicken eggshells. The nanopowders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), particle size distribution (PSD) analyzer, and Fourier transform infrared spectroscopy (FT-IR) techniques. Selected area electron diffraction (SAED) analysis during TEM showed the particles to be polycrystalline in nature. The resulting HA powder exhibited an average size of ~ 35 nm with a narrowly distributed particle size range from 5 to 90 nm. XRD and FT-IR analysis showed that the powders produced were of high purity. The present study provides a simple sol–gel precipitation method to obtain nano HA powders of high purity from biowaste chicken eggshells.     

Electroextraction of boron from boron carbide scrap

Studies were carried out to extract elemental boron from boron carbide scrap. The physicochemical nature of boron obtained through this process was examined by characterizing its chemical purity, specific surface area, size distribution of particles and X-ray crystallite size. The microstructural characteristics of the extracted boron powder were analyzed by using scanning electron microscopy and transmission electron microscopy. Raman spectroscopic examination of boron powder was also carried out to determine its crystalline form. Oxygen and carbon were found to be the major impurities in boron. Boron powder of purity ~ 92 wt. % could be produced by the electroextraction process developed in this study. Optimized method could be used for the recovery of enriched boron (¹⁰B > 20 at. %) from boron carbide scrap generated during the production of boron carbide.     

The role of albumen (egg white) in controlled particle size and electrical conductivity behavior of zinc oxide nanoparticles

The size controlled zinc oxide nanoparticle is synthesized in the isothermal evaporation method with albumen (egg white). This method is simple and cost effective for synthesis of ZnO nano powder. The egg white foam was assisted to increase the reaction rate and produce the zinc oxide nano powder. This method helps to attain the particle size in the range 13-28 nm. The results from X-ray diffraction patterns and TEM micrograph confirmed the formation of nano crystalline phase with particle size ranges from 13 nm to 28 nm. The samples were further analyzed by using Fourier transform Infrared spectroscopy (FT-IR), photoluminescence spectrum (PL), thermogravimetric analysis (TGA) and Resistivity measurement. The less time consumption in isothermal evaporation process was one of the significant roles for large scale zinc oxide nano powder production.     

The role of albumen (egg white) in controlled particle size and electrical conductivity behavior of zinc oxide nanoparticles

The size controlled zinc oxide nanoparticle is synthesized in the isothermal evaporation method with albumen (egg white). This method is simple and cost effective for synthesis of ZnO nano powder. The egg white foam was assisted to increase the reaction rate and produce the zinc oxide nano powder. This method helps to attain the particle size in the range 13–28 nm. The results from X-ray diffraction patterns and TEM micrograph confirmed the formation of nano crystalline phase with particle size ranges from 13 nm to 28 nm. The samples were further analyzed by using Fourier transform Infrared spectroscopy (FT-IR), photoluminescence spectrum (PL), thermogravimetric analysis (TGA) and Resistivity measurement. The less time consumption in isothermal evaporation process was one of the significant roles for large scale zinc oxide nano powder production.     

Improvements of the microstructure and erosion resistance of boron carbide with additives

A series of test materials were produced from boron carbide (B₄C) powders with additions of either boron in amounts up to 60 wt.%, silicon (4 wt.%) or silicon and silicon carbide (4 wt.% and 30 wt.%, respectively). The powder mixtures were densified by encapsulation hot-isostatic pressing. The test materials where evaluated in dry particle erosion tests with silicon carbide grits. Particular attention was given to the relation between the microstructure and the composition.It was found that boron additions up to 20 wt.%, decreased the average grain size and reduced the porosity of the boron carbide. A material with 60 wt.% boron exhibited very low porosity and supreme resistance to particle erosion. The erosion resistance was also significantly improved by additions of silicon and silicon carbide.The favorable effects of boron, silicon and silicon carbide are discussed in terms of their influence on microstructural parameters, such as grain size, porosity, grain boundaries and reduction of free carbon.     

固相反应法合成碳化硼纳米粉体

以六方氮化硼和炭黑(或石墨)为原料, 采用固相反应法合成了碳化硼粉体. 碳源、反应气氛和温度对粉体合成产生重要影响. 以炭黑为碳源, 在1900℃真空下保温5 h, 得到了平均粒径约为100 nm的碳化硼纳米粉体. 与商业粉体相比, 合成的粉体具有较好的烧结活性. 在2000℃/30 MPa/1 h条件下烧结, 样品的相对密度达到97.9%(商业粉体样品为93.1%), 这可归结于合成的粉体具有细小的粒径、低的氧含量和一定程度的孪晶结构.     

Analysis of the compaction behavior of Al–SiC nanocomposites using linear and non-linear compaction equations

The compressibility behavior of Al–SiC nanocomposite powders was examined and the density-pressure data were analyzed by linear and non-linear compaction equations. SiC particles with an average size of 50 nm were mixed with gas-atomized aluminum powder (40 μm average size) at different volume fractions (up to 20 vol%) and compacted in a rigid die at various pressures. In order to highlight the effect of reinforcement particle size, the compressibility of micrometric SiC particles of two sizes (1 and 40 μm) was also examined. Analysis of the compressibility data indicated hindering effect of the hard ceramic particles on the plastic deformability of soft aluminum matrix, particularly at high volume fractions. More pronounced effect on the yield pressure was obtained for the nanometric particles compared with the micrometric ones. Nevertheless, better particles rearrangement was taken place when the ultrafine SiC particles were utilized. In light of the experimental and theoretical analysis, the densification mechanism of aluminum matrix composites and the effect of reinforcement particle size and volume fraction are discussed.     

Facile synthesis of cubic boron nitride nanoparticles from amorphous boron by triple thermal plasma jets at atmospheric pressure

Cubic boron nitride (c-BN) is a superhard material, with hardness value comparable to that of diamond. c-BN is used in a wide range of industrial applications, including tool, abrasives, and refractory. The hardness of c-BN can be improved by decreasing the particle size to the nanoscale; however, the simultaneous application of high pressure (～8 GPa) and temperature (>2,500 K) is required to synthesize the c-BN crystal structure. In this study, we effectively synthesized c-BN nanoparticles from amorphous boron using a triple direct current (DC) thermal plasma jet system at atmospheric pressure. The injection of nitrogen as plasma forming gas generated reactive nitridation species. The average particle size of the synthesized c-BN was 22 nm, and the major crystal structure is the (1 1 1) cubic phase. We carried out a numerical simulation for a thermal fluid, to confirm the high temperature and velocity fields of the plasma jets that formed inside the reactor as the flow rate of plasma forming gas was adjusted. A high production yield of 51% was achieved using amorphous boron at a feed rate of 190 mg/min and the c-BN nanoparticles exhibited high crystallinity without requiring pre-and post-processing.     

The role of various boron precursor on superconducting properties of MgB2/Fe

The superconducting properties of Fe sheathed MgB₂ wire has been studied as a function of precursor B powder particle size. The in situ processed MgB₂ samples were prepared by means of conventional solid state reaction method with magnesium powder (99.8%, 325 mesh) and three different types of amorphous boron powders (purity; 98.8%, >95% and 91.9%) from two sources, Pavezyum (Turkish supplier) and Sigma Aldrich. The particle sizes of Turkish boron precursor powder were selected between 300 and 800 nm. The structural and magnetic properties of the prepared samples were investigated by means of the X-ray powder diffraction (XRD) and ac susceptibility measurements. The XRD patterns showed that the diffraction peaks for our samples belong to the main phase of the MgB₂ diffraction patterns. The highest critical temperature, T_c = 38.4 K was measured for the MgB₂ sample which was fabricated by using the 98.8% B. The critical current density of this sample was extracted from the magnetization measurements and J_c = 5.4 × 10⁵ A cm⁻² at 5 K and B = 2 T. We found that the sample made by using the 98.8% boron showed almost 2 times higher J_c than that of obtained from 91.9% B powder.     

Microstructural evolution during mechanical milling of Ti/Al powder mixture and production of intermetallic TiAl cathode target

Titanium aluminides are of great technological interest because of their attractive mechanical properties. Mechanical milling/alloying is a promising powder metallurgical technique, which can achieve ultrafine, uniform and manipulable microstructures. In this study, we employed a recently revisited discus mill to produce a composite Ti–(50–57) at.%Al powder feedstock, which is suitable for hot consolidation to produce bulk cathode targets for physical vapour deposition (PVD) coatings. The effects of milling time, quantity of process control agent (PCA) and discus-to-powder weight ratio (DPR) on the microstructure evolution of the attendant Ti/Al composite powder were investigated in detail. It was found that to produce Ti/Al composite powders with a fine particle size and a uniform microstructure, the practicable processing parameters should be 2 or 3% isopropanol addition as PCA, 12 h of milling time and at least 13:1 DPR weight ratio. Cathode targets were produced by hot isostatic pressing (HIPing) the as-milled powders. The targets were then used to produce a PVD TiAlN coating which had an average microhardness of 2400 HV.     

Effect of particle size on microstructure and strength of porous spinel ceramics prepared by pore-forming <Emphasis Type="Italic">in situ</Emphasis> technique

The porous spinel ceramics were prepared from magnesite and bauxite by the pore-forming in situ technique. The characterization of porous spinel ceramics was determined by X-ray diffractometer (XRD), scanning electron microscopy(SEM), mercury porosimetry measurement etc and the effects of particle size on microstructure and strength were investigated. It was found that particle size affects strongly on the microstructure and strength. With decreasing particle size, the pore size distribution occurs from multi-peak mode to bi-peak mode, and lastly to mono-peak mode; the porosity decreases but strength increases. The most apposite mode is the specimens from the grinded powder with a particle size of 6·53 μm, which has a high apparent porosity (40%), a high compressive strength (75·6 MPa), a small average pore size (2·53 μm) and a homogeneous pore size distribution.     

Refining of copper powder by a novel micro-abrasive milling method conducted in the air

The pure copper powder was milled by conventional high-energy ball milling (CM) and micro-abrasive milling (MAM) methods in the air or vacuum. The refining behavior of copper powder milled using these different methods has been studied, and the morphologies, microstructures, compositions, and properties of the milled powders have been thoroughly investigated. The results show that, as compared to CM, the MAMed copper powder had a better refinement behavior and contained a smaller number of agglomerates. After milling in the air for 30 h by MAM, whole copper powder was converted into Cu₂₊₁O. In addition, under the synergistic effects of micro-abrasion and exposure to oxygen, the Cu₂₊₁O powder was soft-agglomerated and had a specific surface area of 15.1031 m²/g and an average size of 375.4 nm. During the dispersion process, Cu₂₊₁O was partly converted into CuO and the microstructural evolution characteristics were disclosed. The dispersed powder had an average particle size of 179.5 nm. The refining mechanism of the copper powder prepared by the micro-abrasive milling method was also discussed.     

Nanocrystalline hydroxyapatite doped with magnesium and zinc: Synthesis and characterization

During recent years, there have been efforts in developing nanocrystalline bioceramics, to enhance their mechanical and biological properties for use in tissue engineering applications. In this research, we made an attempt to synthesize nanocrystalline bioactive hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂, HAp) ceramic powder in the lower-end of nano-range (2–10 nm), using a simple low-temperature sol–gel technique and studied its densification behavior. We further studied the effects of metal ion dopants during synthesis on powder morphology, and the properties of the sintered structures. Calcium nitrate and triethyl phosphite were used as precursors for calcium and phosphorous, respectively, for sol–gel synthesis. Calculated quantities of magnesium oxide and zinc oxide were incorporated as dopants into amorphous dried powder, prior to calcination at 250–550 °C. The synthesized powders were analyzed for their phases using X-ray diffraction technique and characterized for powder morphology and particle size using transmission electron microscopy (TEM). TEM analysis showed that the average particle size of the synthesized powders were in the range of 2–10 nm. The synthesized nano-powders were uniaxially compacted and then sintered at 1250 °C and 1300 °C for 6 h, separately, in air. A maximum average sintered density of 3.29 g/cm³ was achieved in structures sintered at 1300 °C, developed from nano-powder doped with magnesium. Vickers hardness testing was performed to determine the hardness of the sintered structures. Uniaxial compression tests were performed to evaluate the mechanical properties. Bioactivity and biodegradation behavior of the sintered structures were assessed in simulated body fluid (SBF) and maintained in a dynamic state.     

Microstructural characterization of P/M Ni3Al consolidated by HIP

Rapidly solidified powder of Ni₃Al doped with boron was produced by inert gas atomization and consolidated by hot isostatic pressing (HIP). Morphology and microstructure of the powder were studied. From the particle morphology, it could be deduced that the solidification time was similar at least to the time necessary for complete fragmentation of the liquid. The powder showed a two-phase microstructure that was finer the smaller the particle size. The presence of dendrites of NiAl (β) phase was consistent with the diagram proposed by Schramm and not with the traditional diagram of Singleton et al. The microstructure of the material consolidated at 1100°C and 1200°C was studied. A monophasic structure was observed after HIP, and no relevant microstructural differences were seen between the two temperatures used.     

Effect of SiC particle size on the physical and mechanical properties of extruded Al matrix nanocomposites

In this work, the effect of SiC particle size and its amount on both physical and mechanical properties of Al matrix composite were investigated. SiC of particle size 70 nm, 10 μm and 40 μm, and Al powder of particle size 60 μm were used. Composites of Al with 5 and 10 wt.% SiC were fabricated by powder metallurgy technique followed by hot extrusion. Phase composition and microstructure were characterized. Relative density, thermal conductivity, hardness and compression strength were studied. The results showed that the X-ray diffraction (XRD) analysis indicated that the dominant components were Al and SiC. Densification and thermal conductivity of the composites decreased with increasing the amount of SiC and increased with increasing SiC particle size. Scanning electron microscope (SEM) studies showed that the distribution of the reinforced particle was uniform. Increasing the amount of SiC leads to higher hardness and consequently improves the compressive strength of Al–SiC composite. Moreover, as the SiC particle size decreases, hardness and compressive strength increase. The use of fine SiC particles has a similar effect on both hardness and compressive strength.     

Impact of powder composition on processing-relevant properties of pharmaceutical materials: An experimental study

In this work, we studied the influence of powder composition on packing density and other processing-relevant properties of binary mixtures, including powder flowability. Binary mixtures of pharmaceutical powders with different particle size ratios, α and varying fractions of large and small particles were analyzed systematically. Mixtures of three excipients and one API with different composition (2, 5, 10, 30, 50, 70, 90, 95 and 98 wt%) were prepared in a Turbula mixer. Powders with different properties and particle size distribution were chosen, in order to obtain three binary mixtures with different size ratios. Then, macroscopic powder properties including bulk (poured) and tapped density (BD and TD) were measured. A powder rheometer was used to measure the flow function coefficient (ffc), cohesion, compressibility and permeability of the binary mixtures. We considered experimentally three classes of binary mixtures, which are characterized by two critical ratios of particle diameter: the critical size ratio of entrance (α_c) and the critical size ratio of replacement (α_r), where α_c = 0.154 and α_r = 0.741. Below the critical size ratio of entrance (α_c), the particle asymmetry (ratio between large and small particle diameters) is high and small particles can fill the voids between larger ones. Between α_c and the critical size ratio of replacement (α_r), the smaller particles are too large to fit in the voids between larger particles (packing structure changes). Above α_r, the particles are more or less symmetric in size and overall packing structure does not change by mixing the particles. Our experiments show that there is a non-linear and non-monotonic dependence of all relevant properties on composition for powder mixtures that have an α < α_r. This non-linear behavior is even more significant for strongly asymmetric binary mixtures with α < α_c. We argue that this behavior is related to the composition dependence of random packing of particulate systems. Our results have relevance to pharmaceutical particle processing operations where constant powder mixture properties are needed to ensure quality standards are met; such operations include capsule or die filling during tableting, and the continuous feeding of powders via screw feeders. Our results suggest that for pharmaceutical particle processing operations, where constant powder mixture properties are a prerequisite for process robustness, the size ratio of API and excipient particles, α should not be smaller than α_r = 0.741.     

A protein powder agglomeration process using açaí pulp as the binder: An analysis of the process parameters

This work investigated the fluidized bed agglomeration of a plant protein powder blend using an açaí pulp binder in order to improve the physical and handling properties. The blend was prepared mixing isolated pea protein powder and concentrated rice protein powder. The influence of air temperature and binder flow rate on the moisture content, particle size and process yield was evaluated using a factorial design. The anthocyanins content, wettability and flowability of the powder was also evaluated. The agglomeration produced large granules with better physical properties, indicating that açaí pulp can be used as a binder. Statistical analysis showed that binder flow rate had the greatest influence on moisture content and process yield; air temperature had a greater effect on particle size. The optimum condition (T = 75 °C, Q = 2.0 mL/min) resulted in granules that were twice as large as the initial particles. Anthocyanins were incorporated (2.34 mg/100 g) with an acceptable moisture content (≤10%) and a high yield (>75%). Flowability was greater in the agglomerated powder than in the raw material with a wetting time reduction of about 77.0%. The resulting protein powder combines the properties of an instant powder with health and nutritional benefits.     

Microwave direct synthesis of MgB2 superconductor

Intermetallic compound superconductor MgB₂ was synthesized from spherical magnesium powder and lower purity amorphous boron powder by microwave direct heating. Powder X-ray diffraction (XRD) analysis indicates that the phases of the synthesis sample are MgB₂ (major phase) and a small amount of MgO. Scanning electron microscope (SEM) observation shows that the MgB₂ grain size is homogeneous and the particle size is about several hundreds of nanometers. The onset superconducting transition temperature of the MgB₂ sample measured by the temperature dependence of magnetization measurement is about 37.6 K. The critical current density J_c calculated according to the Bean model are about 2.0 × 10⁵ A/cm² at 20 K in self-field and 1.0 × 10⁵ A/cm² at 20 K in 1 T applied field.     

Effect of vibro-milling time on phase formation and particle size of lead zirconate nanopowders

A perovskite phase of lead zirconate, PbZrO₃, nanopowder was synthesized by a solid-state reaction via a rapid vibro-milling technique. The effect of milling time on the phase formation and particle size of PbZrO₃ powder was investigated. Powder samples were characterized using TG-DTA, XRD, SEM and laser diffraction techniques. It was found that an average particle size of 50 nm was achieved at 25 h of vibro-milling after which a higher degree of particle agglomeration was observed upon continuation of milling to 35 h. In addition, by employing an appropriate choice of milling time, a narrow particle size distribution curve was also observed.     

Synthesis and luminescence properties of YAG:Ce nanopowder prepared by the Pechini method

Cerium-doped yttrium aluminum garnet (YAG:Ce) powder was synthesized by the Pechini method with aluminum nitride, yttrium nitride, citric acid and ethylene glycol as the starting materials. Structure, morphology and luminescence spectra were investigated by using X-ray diffraction, thermogravimetric and differential thermal analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and photoluminescence spectroscopy measurements. The pure YAG phase was formed after heat treatment at 800 °C for 3 h and no intermediate phase was observed. The average size of the particles was about 70 nm. The photoluminescence spectrum of the crystalline YAG:Ce phosphors showed the green-yellow emission with 5d → 4f transition as the most prominent group.The increase of the ethylene glycol:citric acid molar ratio, resulted in a powder with smaller particle size and better luminescence properties.